Synthesis of new Group III fluoride–ammonia adducts in supercritical ammonia: structures of AlF3(NH3)2 and InF2(NH2)(NH3)

Ketchum, Douglas R.; Schimek, George L.; Pennington, William T.; Kolis, Joseph W.

doi:10.1016/s0020-1693(99)00286-8

Cited by 23 publications

(23 citation statements)

References 25 publications

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“…Similar simultaneous coordination by amide ions and ammonia molecules was previously reported in, for example, KNH 2 ·2NH 3 [5], or more relevant for the discussion, [Cr 2 (NH 2 ) 3 (NH 3 ) 6 ]I 2 [6] and InF 2 (NH 2 )(NH 3 ) [7], both with octahedral coordination at the metal atom and obtained from the respective halides under ammonothermal conditions.…”

Section: Resultssupporting

confidence: 82%

Ammonothermal Synthesis and Crystal Structures of Diamminetriamidodizinc Chloride [Zn2(NH3)2(NH2)3]Cl and Diamminemonoamidozinc Bromide [Zn(NH3)2(NH2)]Br

et al. 2016

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Abstract:The treatment of excess zinc in the presence of ammonium chloride under ammonothermal conditions of 873 K and 97 MPa leads to diamminetriamidodizinc chloride [Zn 2 (NH 3 ) 2 (NH 2 ) 3 ]Cl with a two-dimensionally µ-amido-interconnected substructure. Similar reaction conditions using ammonium bromide instead of the chloride (773 K, 230 MPa) result in diamminemonoamidozinc bromide [Zn(NH 3 ) 2 (NH 2 )]Br with one-dimensional infinite µ-amido-bridged chains. Both compounds were obtained as colorless, very moisture sensitive crystals. Crystal structures and hydrogen bond schemes are analyzed. Raman spectroscopic data of the chloride are reported.

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Section: Resultssupporting

confidence: 82%

Ammonothermal Synthesis and Crystal Structures of Diamminetriamidodizinc Chloride [Zn2(NH3)2(NH2)3]Cl and Diamminemonoamidozinc Bromide [Zn(NH3)2(NH2)]Br

et al. 2016

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“…Interestingly, the triammoniate of iron fluoride, recently obtained from FeF 3 in liquid ammonia, shows no dissociation into differently charged ions in solid state, but it has a mer arrangement of uncharged [FeF 3 (NH 3 ) 3 ] molecules heavily involved in hydrogen bonding 35. On reduction of the ammonia content in the triammoniate Ga(NH 3 ) 3 F 3 to the diammoniate Ga(NH 3 ) 2 F 3 and finally the monoammoniate Ga(NH 3 )F 3 , the octahedral coordination of the Ga centre is preserved, but the octahedra are connected by fluoride ligands to form infinite chains of trans ‐[Ga(NH 3 ) 2 F 2 F 2/2 ] or layers of [Ga(NH 3 )FF 4/2 ], respectively 9…”

Section: Resultsmentioning

confidence: 99%

“…Ammoniates of aluminum halides can be formed in supercritical ammonia in the presence of AlN and NH 4 F9 or only aluminum halides10 as starting materials. These compounds are expected to be potential inorganic precursors for the synthesis of AlN by thermal decomposition under certain conditions.…”

Section: Introductionmentioning

confidence: 99%

Intermediates in Ammonothermal GaN Crystal Growth under Ammonoacidic Conditions

et al. 2013

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Crystals of two new hexammoniates, namely, [Ga(NH3)6]I3·NH3 and [Ga(NH3)6]Br3·NH3, were grown from liquid ammonia solutions of GaI3 and GaBr3 in a wide temperature range. The known compound [Ga(NH3)5Cl]Cl2 and the new triammoniate of gallium fluoride Ga(NH3)3F3 were obtained ammonothermally during the synthesis of GaN from NH4Cl and NH4F, respectively. The compounds are characterized by crystallographic parameters derived from their X‐ray diffraction data. The crystal structures of all the ammoniates feature octahedrally coordinated Ga atoms in complex ions of the general form [Ga(NH3)6–nXn](3–n)+ (n = 0, 1, 2, 4; X = F, Cl, Br, I). The extensive N–H···X hydrogen bonding networks in these compounds are analyzed. The IR and Raman spectroscopy data for [Ga(NH3)6]X3·NH3 (X = Br, I) and Ga(NH3)2F3 are provided, and the IR spectrum of Ga(NH3)3F3 is compared with those published for the monoammoniate Ga(NH3)F3 and the diammoniate Ga(NH3)2F3. Finally, the thermal deamination features of [Ga(NH3)6]X3·NH3 (X = Br, I) and Ga(NH3)3F3 are also discussed.

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“…[7,8] Particularly, amides, ammoniates and ammine adducts of indium have barely been discussed in literature. [9][10][11] Early attempts yielded In(NH 2 ) 3 among other compounds. [9] Ketchum et al obtained InF 2 (NH 2 )(NH 3 ) with a layered crystal structure from InN and NH 4 F under ammonothermal conditions.…”

Section: Introductionmentioning

confidence: 99%

“…[9] Ketchum et al obtained InF 2 (NH 2 )(NH 3 ) with a layered crystal structure from InN and NH 4 F under ammonothermal conditions. [10] Bremm et al were able to synthesize In(NH 3 ) 3 Cl 3 , featuring octahedral [In(NH 3 ) 4 Cl 2 ] + and [In(NH 3 ) 2 Cl 4 ] À ions and showing close structural similarity to Ga(NH 3 ) 3 F 3 , which was observed in ammonoacidic GaN synthesis. [11,12] In contrast to the analogue ammoniates and amides of gallium, the isolation and characterization of indium amides and ammoniates proved to be challenging, due to the rather labile bond between indium and nitrogen, also expressed in the metastable nature of binary indium nitride.…”

Section: Introductionmentioning

confidence: 99%

Two Intermediates in Ammonothermal InN Crystal Growth: [In(NH₃)₅Cl]Cl₂ and InF₂(NH₂)

Becker

Cekovski

Niewa

2021

Zeitschrift anorg allge chemie

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The ammonothermal synthesis is a promising instrument for synthesis and crystal growth of the metastable semiconductor InN. Two novel intermediates within the ammonothermal InN crystal growth have been synthesized, namely pentaamminechloridoindium dichloride, [In(NH 3 ) 5 Cl]Cl 2 , and indium amide difluoride, InF 2 (NH 2 ). Both intermediates were obtained under ammonothermal conditions (T max = 663 K, p max = 118.3 MPa, and T max = 753 K, respectively) in a near-ammononeutral milieu as established for InN crystal growth, using the respective indium trihalide together with potassium amide as mineralizer system.The crystal structure of [In(NH 3 ) 5 Cl]Cl 2 shows strong structural relations to the corresponding intermediate [Ga(NH 3 ) 5 Cl]Cl 2 within ammonoacidic GaN crystal growth. At ambient pressure, it decomposes above 450 K under release of ammonia. InF 2 (NH 2 ) shows attributes of a classical MX 3 crystal structure, realizing the motif of a hexagonal close packing of (NH) 2 À together with F À ions and indium occupying one third of the octahedral holes between every layer of the packing. Vibrational spectroscopy for both solid intermediates is reported.

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Synthesis of new Group III fluoride–ammonia adducts in supercritical ammonia: structures of AlF3(NH3)2 and InF2(NH2)(NH3)

Cited by 23 publications

References 25 publications

Ammonothermal Synthesis and Crystal Structures of Diamminetriamidodizinc Chloride [Zn2(NH3)2(NH2)3]Cl and Diamminemonoamidozinc Bromide [Zn(NH3)2(NH2)]Br

Ammonothermal Synthesis and Crystal Structures of Diamminetriamidodizinc Chloride [Zn2(NH3)2(NH2)3]Cl and Diamminemonoamidozinc Bromide [Zn(NH3)2(NH2)]Br

Intermediates in Ammonothermal GaN Crystal Growth under Ammonoacidic Conditions

Two Intermediates in Ammonothermal InN Crystal Growth: [In(NH₃)₅Cl]Cl₂ and InF₂(NH₂)

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Synthesis of new Group III fluoride–ammonia adducts in supercritical ammonia: structures of AlF3(NH3)2 and InF2(NH2)(NH3)

Cited by 23 publications

References 25 publications

Ammonothermal Synthesis and Crystal Structures of Diamminetriamidodizinc Chloride [Zn2(NH3)2(NH2)3]Cl and Diamminemonoamidozinc Bromide [Zn(NH3)2(NH2)]Br

Ammonothermal Synthesis and Crystal Structures of Diamminetriamidodizinc Chloride [Zn2(NH3)2(NH2)3]Cl and Diamminemonoamidozinc Bromide [Zn(NH3)2(NH2)]Br

Intermediates in Ammonothermal GaN Crystal Growth under Ammonoacidic Conditions

Two Intermediates in Ammonothermal InN Crystal Growth: [In(NH3)5Cl]Cl2 and InF2(NH2)

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Two Intermediates in Ammonothermal InN Crystal Growth: [In(NH₃)₅Cl]Cl₂ and InF₂(NH₂)